TWI503175B - Low-pressure milling process - Google Patents

Description

低壓研磨製程Low pressure grinding process

本發明關於一種新穎的噴射研磨機、利用噴射研磨機產生細粒子之製程、該細粒子的同步表面改質之製程及亦關於由此製程所產製之產物。The present invention relates to a novel jet mill, a process for producing fine particles by a jet mill, a process for synchronizing surface modification of the fine particles, and a product produced by the process.

在利用噴射研磨機執行研磨操作時，欲研磨及/或欲分級之材料包含相對粗及相對細的粒子，該等粒子夾帶在空氣流中且形成產物流，可將該產物流引入噴射研磨機的空氣分級器之容箱中。產物流係以徑向方向前進至空氣分級器之分級輪中。在分級輪中，相對粗的粒子與空氣流分離且空氣流離開分級輪，細粒子以軸向通過外流管。接著將欲濾出或欲產製之具有細粒子的空氣流饋入過濾器中，使流體(諸如空氣)及細粒子於過濾器中彼此分離。When the grinding operation is performed using a jet mill, the material to be ground and/or to be classified contains relatively coarse and relatively fine particles which are entrained in the air stream and form a product stream which can be introduced into the jet mill The air classifier is in the box. The product stream is advanced in the radial direction into the classifier wheel of the air classifier. In the classifying wheel, the relatively coarse particles are separated from the air stream and the air stream exits the classifying wheel, the fine particles passing axially through the outflow tube. The air stream having fine particles to be filtered out or to be produced is then fed into the filter to separate fluids (such as air) and fine particles from each other in the filter.

DE 198 24 062 A1揭示一噴射研磨機，其研磨室中額外有至少一種高能量熱蒸汽研磨噴射流以高流動能量引入，除了具有用於至少一種研磨噴射流的入口裝置以外尚具有用於待研磨材料的入口及用於產物的出口之研磨室，及在待研磨材料與至少一種熱蒸汽研磨噴射流一起來到的區域中待研磨材料具有至少大致相同的溫度。DE 198 24 062 A1 discloses a jet mill in which at least one high-energy hot steam grinding jet is additionally introduced in the grinding chamber with high flow energy, in addition to having an inlet device for at least one abrasive jet, The inlet of the abrasive material and the grinding chamber for the outlet of the product, and the material to be ground in the region where the material to be abraded comes together with the at least one hot steam abrasive jet has at least substantially the same temperature.

此外，對應之空氣分級器(特別用於噴射研磨機)係由例如EP 0 452 930 B1所揭示。此空氣分級器及其操作方式原則上非常令人滿意。Furthermore, corresponding air classifiers (especially for jet mills) are disclosed, for example, in EP 0 452 930 B1. This air classifier and its mode of operation are in principle very satisfactory.

前述製程具有彼等僅可以高經費裝置操作，而且非常耗費能量的缺點。為了使此問題減至最低，DE 10 2006 023 193提出其中使研磨壓力下降至4.5巴以下之製程。此製程更具能量效率，但是具有如以前一樣的操作介質(研磨氣體)溫度高的缺點。用於產生操作介質的壓力及操作介質的溫度之DE 10 2006 023 193提及例如DE 198 24 062或提出使用壓縮機。The aforementioned processes have the disadvantage that they can only be operated with high cost and are very energy intensive. In order to minimize this problem, DE 10 2006 023 193 proposes a process in which the grinding pressure is reduced below 4.5 bar. This process is more energy efficient, but has the disadvantage that the operating medium (grinding gas) has a high temperature as before. DE 10 2006 023 193, which is used for the production of the pressure of the operating medium and the temperature of the operating medium, is mentioned, for example, in DE 198 24 062 or the use of a compressor.

已知使用機械或分級機械研磨機作為噴射研磨機的替代品。然而，由於與轉子/定子直接接觸而使該等研磨機具有待研磨材料在研磨機上造成重大磨耗的缺點。此進而導致研磨機的高保養成本，但同時亦從研磨導致不希望的材料污染。It is known to use mechanical or fractional mechanical grinders as an alternative to jet mills. However, such grinders have the disadvantage of causing significant wear on the grinder due to the direct contact with the rotor/stator. This in turn leads to a high maintenance cost of the grinding machine, but at the same time leads to undesired material contamination from the grinding.

本發明之目的因此係提供儘可能具能量效率且從研磨導致與以機械或分級機械研磨機研磨相比而較低的材料污染之研磨製程。在特定的目的中，目標係從新式製程研磨之材料的粒度分布至少等於或比以機械或分級機械研磨機之研磨製程的例子中更好的粒度分布。It is therefore an object of the present invention to provide a grinding process that is as energy efficient as possible and that results in lower material contamination from grinding than in mechanical or fractional mechanical mill grinding. For a particular purpose, the particle size distribution of the material targeted to be ground from the new process is at least equal to or better than the particle size distribution of the example of the mechanical process of a mechanical or fractional mechanical mill.

本發明之特定目的係提供儘可能具能量效率且從研磨導致與以機械或分級機械研磨機研磨相比而較低的材料污染之研磨製程，且使此製程有可能在研磨期間進行待研磨材料之表面改質(例如，塗佈、摻雜)。A particular object of the present invention is to provide a grinding process that is as energy efficient as possible and that results in lower material contamination from grinding than mechanical or fractional mechanical mill grinding, and that makes it possible to carry out the material to be ground during grinding. Surface modification (eg, coating, doping).

進一步的目的係提供新穎的粉狀材料，其具有例如鐵的低污染。A further object is to provide novel powdered materials which have low contamination such as iron.

未明確述及之更多目的係從以下的說明、申請專利範圍、實例和圖式的整個上下文浮現。Further objects that are not explicitly mentioned are apparent from the following description, the scope of the patent application, the examples and the drawings.

先前述及之目的係由申請專利範圍、以下的說明、實例和圖式中更詳細定義之製程及由其中更詳細定義之產物達成。The foregoing and other objects are achieved by the scope of the patent application, the following description, examples and drawings, and the more detailed definitions thereof.

本發明者驚訝地發現有可能在噴射研磨機中以低於4巴之壓力及低於100℃之溫度下研磨無機及有機材料，以此一方式使彼等隨後具有至少對應於若以相同材料在具有轉子/定子(分級及未分級)之研磨機中研磨時所獲得的粒子範圍。因此可產製具有相同的粒子範圍，但較低的雜質含量之產物。The inventors have surprisingly found that it is possible to grind inorganic and organic materials in a jet mill at a pressure of less than 4 bar and a temperature of less than 100 ° C, in such a way that they subsequently have at least corresponding to the same material. The range of particles obtained when grinding in a grinder with rotor/stator (classified and ungraded). It is therefore possible to produce products having the same particle range but lower impurity content.

然而，由於溫和的研磨條件，亦有可能以根據本發明之製程產製具有減少的細料含量及/或因此具有與機械研磨機相比而較窄的粒子大小分布之粒子。However, due to the mild milling conditions, it is also possible to produce particles having a reduced fines content and/or thus a narrower particle size distribution compared to a mechanical mill in accordance with the process of the present invention.

此外，本發明者發現在此製程的例子中有可能在與研磨的同時間進行待研磨粒子的塗佈或摻雜。此特別值得述及，因為在機械或分級機械研磨機中不可能在與研磨的同時間進行塗佈或摻雜，因為結塊通常發生在研磨機的轉子/定子/壁上及因為在根據本發明之製程中的溫度和壓力非常低。Furthermore, the inventors have found that in the example of this process it is possible to carry out the coating or doping of the particles to be ground at the same time as the grinding. This is particularly noteworthy because it is not possible to coat or dope at the same time as grinding in a mechanical or fractional mechanical mill, since agglomeration usually occurs on the rotor/stator/wall of the mill and because The temperature and pressure in the process of the invention are very low.

低壓和低溫亦使此製程有可能使用溫度敏感性表面改質劑且使此製程有可能研磨待研磨之溫度敏感性材料，諸如糖，其不可能用於先前技藝之噴射研磨製程的例子中。Low pressure and low temperature also make it possible to use temperature sensitive surface modifiers and make it possible to grind the temperature sensitive materials to be ground, such as sugar, which is not possible in the prior art example of jet milling processes.

此外，值得述及的是根據本發明之乾式研磨及塗佈製程在溫和條件下有可能產製不可能以已知的製程產製之產物。例如，矽石的研磨及以聚矽氧聚醚丙烯酸酯聚合物的同步塗佈是可能的，且不會損失聚醚含量。就產製的理由而言，該等聚合物有時具有10-20重量%過量之聚醚。頃發現此過量在傳統的濕式研磨的例子中被部分洗出。另一方面，在根據本發明之乾式研磨製程的例子中保留過量聚醚，使得可產製完全不同的矽石粒子塗佈。此導致改進的粒子應用性質。然而，另一方面，新式製程亦具有生態及經濟優勢，因為可顯著地減低或甚至避免流出物的聚醚污染。Furthermore, it is worth mentioning that the dry grinding and coating process according to the present invention makes it possible to produce products which are impossible to produce in a known process under mild conditions. For example, grinding of vermiculite and simultaneous coating with a polyoxyl acrylate polymer are possible without loss of polyether content. For reasons of production, the polymers sometimes have an excess of 10-20% by weight of the polyether. This excess was found to be partially washed out in the conventional wet grinding example. On the other hand, in the example of the dry milling process according to the present invention, excess polyether is retained so that completely different vermiculite particle coatings can be produced. This leads to improved particle application properties. On the other hand, however, the new process also has ecological and economic advantages because it can significantly reduce or even avoid polyether contamination of the effluent.

特別在研磨高磨耗固體的例子中，例如牙齒護理，根據本發明之製程具有特別的優勢。該等物質造成在研磨機上特別大量的磨耗物質，且同時用於人類及動物美容治療之產品必須符合關於雜質含量的高需求。Particularly in the case of grinding high wear solids, such as dental care, the process according to the invention has particular advantages. These materials cause a particularly large amount of abrasive material on the mill, and products for both human and animal cosmetic treatments must meet high demands on the level of impurities.

本發明之主題因此為一種利用噴射研磨機產生細粒子之製程，其特徵在於研磨氣體具有≦4巴之壓力(絕對)及低於100℃之溫度。The subject of the invention is therefore a process for producing fine particles by means of a jet mill, characterized in that the grinding gas has a pressure of ≦4 bar (absolute) and a temperature below 100 °C.

本發明之主題亦為一種利用使用壓縮氣體作為研磨氣體的噴射研磨機(1)產生細粒子之製程，其特徵在於研磨氣體具有≦4巴之壓力(絕對)及低於100℃之溫度，且其特徵在於塗料或摻雜劑係在研磨期間以待研磨材料之粒子的至少部分表面以塗料或摻雜劑覆蓋的此一方式添加。The subject of the invention is also a process for producing fine particles by using a jet mill (1) using a compressed gas as a grinding gas, characterized in that the grinding gas has a pressure of ≦4 bar (absolute) and a temperature lower than 100 ° C, and It is characterized in that the coating or dopant is added during the grinding in such a way that at least part of the surface of the particles of the material to be ground is covered with a coating or a dopant.

本發明之主題同樣為一種噴射研磨機，優先選擇為流化床對向噴射研磨機或密相床噴射研磨機或橢圓管研磨機或螺旋管噴射研磨機，其特徵在於使用鼓風機產生操作介質之壓力，優先選擇為旋轉式鼓風機或徑向式鼓風機。The subject of the invention is likewise a jet mill, preferably a fluidized bed counter jet mill or a dense bed jet mill or an elliptical tube mill or a spiral tube jet mill, characterized in that an operating medium is produced using a blower. Pressure, preferably a rotary blower or a radial blower.

根據本發明之製程代表與先前技藝之製程相比為能量相當優化之製程(低壓力、低溫度、低研磨機磨損、減低的裝置經費)。The process according to the present invention represents a process that is relatively energy-optimized compared to prior art processes (low pressure, low temperature, low grinder wear, reduced device expense).

根據本發明且優先選擇用於根據本發明之製程中的噴射研磨機具有超越先前技藝之噴射研磨機的極大優勢，該優勢在於不需要壓縮機或壓力容器以產生操作介質之壓力和溫度，但卻可使用簡式鼓風機，較佳為旋轉式鼓風機或徑向式鼓風機。此相當地減低裝置經費、降低採購成本及減低保養成本。保養成本亦可藉由在根據本發明之製程中所使用之低溫及低壓而減低。The advantage of the jet mill according to the invention and preferred for use in the process according to the invention has a great advantage over prior art jet mills in that no compressor or pressure vessel is required to generate the pressure and temperature of the operating medium, but However, a simple blower can be used, preferably a rotary blower or a radial blower. This considerably reduces equipment costs, reduces procurement costs and reduces maintenance costs. Maintenance costs can also be reduced by the low temperatures and low pressures used in the process according to the invention.

根據本發明之製程的進一步優勢在於此製程可以已存在的噴射研磨機進行。A further advantage of the process according to the invention is that the process can be carried out with an existing jet mill.

以根據本發明之製程研磨之產物的粒度分布，特別為d₅₀ 值可以類似於利用機械或分級機械研磨機所獲得的粒度分布設定。然而，由於更有效的能量轉換，可使根據本發明研磨之材料中的細料含量與利用機械或分級機械研磨機研磨相比而顯著減少。結果，根據本發明之待研磨材料具有顯著改進之應用性質，例如減低之增稠效應。根據本發明之待研磨材料的進一步優勢為其受到研磨機之磨耗產物的污染與以機械或分級機械研磨機所產生之經研磨材料相比而顯著更少。此非常有利，特別在必須具有高純度之產物的例子中。The particle size distribution of the product ground in accordance with the process of the present invention, particularly the d ₅₀ value, can be similar to the particle size distribution setting obtained with a mechanical or fractional mechanical mill. However, due to more efficient energy conversion, the fines content in the materials ground according to the present invention can be significantly reduced as compared to grinding using mechanical or fractional mechanical mills. As a result, the material to be ground according to the invention has significantly improved application properties, such as reduced thickening effects. A further advantage of the material to be abraded according to the invention is that it is significantly less contaminated by the abrasive product of the mill than the abrasive material produced by a mechanical or fractional mechanical mill. This is very advantageous, especially in the case of products which must have high purity.

如上所述，根據本發明之製程有可能使待研磨材料的塗佈或摻雜與研磨一起進行。此是有利，亦特別因為此塗佈或摻雜可在低於100℃之低溫下執行且因此可使用溫度敏感之塗料或摻雜劑或待研磨材料(例如，糖、三羥甲基丙烷、TegoRad 2300等)。As described above, the process according to the present invention makes it possible to carry out coating or doping of the material to be ground together with the grinding. This is advantageous, in particular because this coating or doping can be carried out at temperatures below 100 ° C and therefore temperature sensitive coatings or dopants or materials to be grounded (eg sugar, trimethylolpropane, Tego Rad 2300, etc.).

根據本發明之製程代表溫和的研磨製程，以其主要保留待研磨材料之物理化學性質，諸如DBP吸收。The process according to the invention represents a mild grinding process in which it primarily retains the physicochemical properties of the material to be ground, such as DBP absorption.

最後，可述及為優勢的是可廣為使用根據本發明之製程，亦即用於有機物質及無機物質二者。在此方式中，此製程不同於例如以DE 10 2006 023 193所述之製程，其僅可用於特定的無機物質。Finally, it can be mentioned that it is advantageous to use the process according to the invention, i.e. for both organic and inorganic substances. In this way, the process differs from the process described, for example, in DE 10 2006 023 193, which can only be used for specific inorganic substances.

將申請案的目的詳細解釋於下。The purpose of the application is explained in detail below.

本發明之較佳及/或有利的改善整體來看係從申請專利範圍及其組合以及從本申請案文件浮現。The preferred and/or advantageous improvements of the present invention as a whole are apparent from the scope of the patent application and combinations thereof and from the present document.

本發明係以下述之示例性具體例及應用實例為基準更詳細解釋且僅以實例方式表現於圖式中，亦即本發明不受限於該等示例性具體例及應用實例或在個別的示例性具體例及應用實例內之特色的各自組合。製程及裝置特色亦分別以類似方式從裝置及製程的說明浮現。The present invention is explained in more detail on the basis of the following specific examples and application examples, and is only shown by way of example in the drawings, that is, the invention is not limited to the exemplary embodiments and application examples or in individual Each of the exemplary embodiments and combinations of features within the application examples. The process and device features also appear in a similar manner from the description of the device and process.

與實際的示例性具體例有關的具體化及/或表現之個別特色不受限於該等示例性具體例或與該等示例性具體例的其他特色之組合，但是可與在技術可行性限制範圍內的任何其他變型組合，即使彼等未於本發明的文件中單獨討論。The individual features of the specificization and/or performance relating to the actual exemplary embodiments are not limited by the exemplary embodiments or combinations of other features of the exemplary embodiments, but may be limited in technical feasibility. Any other variant combinations within the scope, even if they are not separately discussed in the documents of the present invention.

在個別的圖中及圖式的圖解中之相同編號表示相同或類似的組件或具有相同或類似效果的組件。未提供編號的特徵亦從圖式中之圖像明瞭，不論該等特徵是否說明於下。另一方面，內含於本發明的說明中，但是不可見於或表現於圖式中之特徵亦可由熟習本技藝者輕易理解。The same reference numerals in the various figures and the drawings of the drawings represent the same or similar components or components having the same or similar effects. Features that are not provided with numbers are also apparent from the images in the drawings, whether or not such features are described below. On the other hand, the features contained in the description of the present invention, but not visible or expressed in the drawings, can be easily understood by those skilled in the art.

在利用噴射研磨機產生細粒子之製程例子中，由本發明所提供之新式步驟如此明確且可理解，使得不需要以圖式表現個別步驟。In the example of a process for producing fine particles using a jet mill, the novel steps provided by the present invention are so clear and understandable that it is not necessary to represent individual steps in the drawings.

根據本發明之製程為一種利用使用壓縮氣體作為研磨氣體的噴射研磨機產生細粒子之製程，其特徵在於研磨氣體具有≦4巴之壓力(絕對)及低於100℃之溫度。The process according to the present invention is a process for producing fine particles by a jet mill using a compressed gas as a grinding gas, characterized in that the grinding gas has a pressure of ≦4 bar (absolute) and a temperature lower than 100 °C.

該製程較佳地藉由低於或等於95℃，優先選擇低於或等於90℃，特別優先選擇低於或等於80℃，且最特別優先選擇從15至80℃之研磨氣體溫度來進一步發展。在第一個特定較佳的變型中，研磨氣體的溫度為50至80℃，而在第二個特定較佳的變型中，其為15至50℃。研磨氣體的溫度係在研磨氣體進入研磨機中的入口測量。Preferably, the process is further developed by a temperature of less than or equal to 95 ° C, preferably less than or equal to 90 ° C, particularly preferably less than or equal to 80 ° C, and most particularly preferably from 15 to 80 ° C. . In a first particularly preferred variant, the temperature of the grinding gas is from 50 to 80 ° C, and in the second particularly preferred variant it is from 15 to 50 ° C. The temperature of the grinding gas is measured at the inlet of the grinding gas into the mill.

研磨氣體的壓力較佳地低於3巴，特別優先選擇低於2巴，最特別優先選擇低於1巴，特定優先選擇為0.5至1巴，且最特定優先選擇為0.15至0.5巴。The pressure of the grinding gas is preferably below 3 bar, particularly preferably below 2 bar, most particularly preferably below 1 bar, with a specific preference of 0.5 to 1 bar, and most particularly preferably 0.15 to 0.5 bar.

研磨氣體壓力與溫度的以下組合特別佳：0.15至0.5巴與15至50℃及0.15至0.5巴與50至80℃。此組合的實例為0.3巴與20℃及0.4巴與75℃之組合。The following combinations of grinding gas pressure and temperature are particularly preferred: 0.15 to 0.5 bar and 15 to 50 ° C and 0.15 to 0.5 bar and 50 to 80 ° C. An example of such a combination is 0.3 bar in combination with 20 ° C and 0.4 bar and 75 ° C.

在根據本發明之製程中可研磨有機物質及無機物質二者。有機物質的實例為碳水化合物(例如，糖)及羧甲基纖維素。Both organic and inorganic materials can be ground in the process according to the invention. Examples of organic substances are carbohydrates (for example, sugars) and carboxymethylcellulose.

較佳的無機物質為非晶形及結晶狀無機固體。結晶狀無機固體優先選擇為二氧化鈦、氧化鋁及碳酸鈣，而非晶形固體優先選擇為凝膠，但亦為其他類型的非晶形固體。亦較佳的是非晶形及結晶狀無機固體，諸如陶瓷(例如，經燒結之陶瓷)。特別優先選擇彼等為含有或包含至少一種金屬及/或金屬氧化物之固體，特別為元素週期表的第三及第四主族之金屬的非晶形氧化物。此適用於具有不同的結構種類之凝膠及非晶形固體。特別佳的是沉澱矽石、熱解矽石、矽酸鹽、鋁矽酸鹽、電弧矽石(例如，來自Quarzwerke GmbH之Amosil)、玻璃及矽膠，矽膠不僅包含水凝膠，亦包含氣凝膠及乾凝膠。Preferred inorganic materials are amorphous and crystalline inorganic solids. The crystalline inorganic solids are preferably selected from the group consisting of titanium dioxide, aluminum oxide and calcium carbonate, while the amorphous solids are preferably selected as gels, but are also other types of amorphous solids. Also preferred are amorphous and crystalline inorganic solids such as ceramics (e.g., sintered ceramics). It is especially preferred that they are amorphous oxides of metals containing or comprising at least one metal and/or metal oxide, in particular metals of the third and fourth main groups of the Periodic Table of the Elements. This applies to gels and amorphous solids with different structural types. Particularly preferred are precipitated vermiculite, pyrolytic vermiculite, niobate, aluminosilicate, arc meteorite (for example, Amosil from Quarzwerke GmbH), glass and silicone, which contain not only hydrogels but also aerogels. Glue and xerogel.

較佳地以流化床對向噴射研磨機或密相床噴射研磨機用於根據本發明之製程中。Preferably, a fluidized bed opposed jet mill or a dense bed jet mill is used in the process according to the invention.

原則上，可使用在操作條件下為氣體的任何物質或物質混合物作為形成欲引入之研磨噴射流的操作介質，術語操作介質與術語研磨氣體在本發明之範圍內係以同義使用。特別優先選擇使用空氣及/或氫氣及/或氬氣及/或惰性氣體，諸如氦氣及/或氮氣及/或所述操作介質之混合物。以空氣最特別佳。使用惰化氣體較佳，特別在研磨待研磨之氧化敏感性或有機材料時。In principle, any substance or mixture of substances which are gaseous under the operating conditions can be used as the operating medium for forming the abrasive jet to be introduced, the term operating medium and the term abrasive gas being used synonymously within the scope of the invention. Particular preference is given to using air and/or hydrogen and/or argon and/or inert gases, such as helium and/or nitrogen and/or mixtures of said operating medium. The best air is best. It is preferred to use an inerting gas, particularly when grinding the oxidation sensitive or organic material to be ground.

諸如存在於習知的噴射研磨裝置中之壓力槽(但亦為壓縮器)可用於例如形成研磨噴射流。然而，在本發明特定的具體例中，研磨噴射流的壓力係利用鼓風機產生，特別優先選擇利用旋轉式鼓風機或徑向式風扇。結果，可顯著降低研磨裝置的投資成本及操作和保養成本二者。以鼓風機產生研磨噴射流的此特定之新式噴射研磨機為本發明的主題。Pressure tanks (but also compressors) such as those found in conventional jet milling devices can be used, for example, to form a jet jet. However, in a particular embodiment of the invention, the pressure of the abrasive jet is produced using a blower, with a preferred preference being made to utilize a rotary blower or a radial fan. As a result, both the investment cost of the grinding apparatus and the operation and maintenance costs can be significantly reduced. This particular new jet mill, which produces a jet stream with a blower, is the subject of the present invention.

亦優先選擇將噴射研磨機與分級器連接。該分級器可為內分級器或外分級器。特別優先選擇使用整合至噴射研磨機中的動態空氣分級器。關於此點，亦最優先選擇提供空氣分級器包括具有固定或隨半徑減少而增加之淨高的分級轉子或分級輪，使得操作期間流經的分級轉子或輪的表面積至少大致固定。另一選擇或另外，亦可提供使空氣分級器包括具有浸沒管的分級轉子或分級輪，該浸沒管係以分級轉子或分級輪旋轉時隨著其一起旋轉的方式設計。It is also preferred to connect the jet mill to the classifier. The classifier can be an inner classifier or an outer classifier. It is particularly preferred to use a dynamic air classifier integrated into the jet mill. In this regard, it is also most preferred to provide the air classifier including a staged or graded wheel having a net height that is fixed or increased with decreasing radius such that the surface area of the staged rotor or wheel flowing through during operation is at least substantially fixed. Alternatively or additionally, it is also possible to provide an air classifier comprising a classifying rotor or a grading wheel having a immersion tube designed to rotate with the grading rotor or the grading wheel as they rotate together.

製程進一步的較佳改善在於提供細料出口室，其具有在流動方向上變寬的橫截面。A further preferred improvement of the process consists in providing a fines outlet chamber having a cross section that widens in the direction of flow.

在圖1中，以示意圖表現用於進行以上解釋之製程的噴射研磨機1之示例性具體例。如上所述，根據本發明之製程可以熟習本技藝者以其本身已知的設備及設施輕易地實現，雖然不意欲以其暗示熟習本技藝者亦可能知道由本發明新開創之製程的個別步驟。In Fig. 1, an exemplary embodiment of the jet mill 1 for performing the above explained process is schematically shown. As described above, the process in accordance with the present invention can be readily implemented by those skilled in the art from the equipment and facilities known per se, although it is not intended to suggest that the skilled person will be aware of the individual steps of the process pioneered by the present invention.

根據圖1之噴射磨機1包括圍住研磨室3的圓筒狀容箱2、約為研磨室3一半高度的待研磨材料之進料4、至少一個在研磨室3下方區域中之研磨噴射入口5及在研磨室3上方區域中之產物出口6。在此配置具有可旋轉之分級輪8的空氣分級器7，經研磨材料(未顯示)以此分級器分級，以便經由產物出口6自研磨室3只排放小於特定粒度之經研磨材料，且反饋具有大於選擇值之粒度的經研磨材料，供進一步研磨操作。The jet mill 1 according to Fig. 1 comprises a cylindrical tank 2 surrounding the grinding chamber 3, a feed 4 of material to be ground which is about half the height of the grinding chamber 3, and at least one grinding jet in the area below the grinding chamber 3. The inlet 5 and the product outlet 6 in the area above the grinding chamber 3. Here, an air classifier 7 having a rotatable classifying wheel 8 is arranged, which is graded by means of an abrasive material (not shown) in order to discharge only the ground material of less than a specific particle size from the grinding chamber 3 via the product outlet 6 and the feedback An abrasive material having a particle size greater than a selected value for further grinding operations.

分級輪8可為慣常用於空氣分級器中之分級輪，其葉片(參考下文，例如與圖3有關)限定徑向延伸之葉片通道，分級空氣在通道外端進入，且相對小粒度或質量之粒子被夾帶至中心出口及產物出口6，而相對大的粒子或相對大質量之粒子在離心力的影響下偏離。空氣分級器7且/或至少其分級輪8特別具備有至少一種根據BP 0 472 930 B1之設計特色。The grading wheel 8 can be a grading wheel conventionally used in an air classifier, the blades of which (referred to below, for example in connection with Figure 3) define radially extending vane passages, the grading air entering at the outer end of the passage, and having a relatively small grain size or mass The particles are entrained to the central outlet and the product outlet 6, while relatively large particles or relatively large particles deviate under the influence of centrifugal force. The air classifier 7 and/or at least its classifying wheel 8 is in particular provided with at least one design feature according to BP 0 472 930 B1.

可能只提供一個待研磨材料入口5，例如包含單一徑向導入口孔或入口噴嘴9，以便使單一研磨噴射流10以高能量碰撞從待研磨材料之進料4到達研磨噴射流10區域的待研磨材料粒子，且使待研磨材料粒子破裂成更小的亞微粒子，將此亞微粒子以分級輪8吸入，且若其具有適當的小尺寸或質量時，則經由產物出口6運送出來。然而，以配對之相反對立的待研磨材料入口5達到更好的效果，其形成兩個彼此相撞的研磨噴射流10，其引起比只有可能以一個研磨噴射流10更強的粒子破裂，特別若產生許多個配對的研磨噴射流時。It is possible to provide only one material inlet 5 to be ground, for example comprising a single radial inlet orifice or inlet nozzle 9 in order to cause a single abrasive jet 10 to collide with high energy from the feed 4 of the material to be ground to the area of the abrasive jet 10 The particles of the material are ground and the particles of the material to be abraded are broken into smaller submicron particles, which are aspirated by the classifying wheel 8, and if they have a suitable small size or mass, are transported through the product outlet 6. However, a better effect is achieved with the oppositely opposed inlets 5 of the material to be abraded, which form two abrasive jets 10 which collide with each other, which cause cracking of the particles which is stronger than only one of the abrasive jets 10, in particular If a plurality of matched abrasive jets are produced.

此外，有可能例如使處理溫度受到以下的影響：在待研磨材料之進料4與研磨噴射流10區域之間使用內部加熱源11或在待研磨材料之進料4外部區域內使用對應之加熱源12，或處理待研磨材料粒子，該粒子在任何情況中皆已溫熱，其避免在進入待研磨材料之進料4時的熱損失，就此目的而將饋料管13以溫度隔絕套14環繞。加熱源11或12(若使用時)原則上可為任何所欲種類，且因此適合特定用於意欲目的及根據市場上的可取得性來選擇，所以不需要關於此點的進一步解釋。Furthermore, it is possible, for example, to have the treatment temperature affected by the use of an internal heating source 11 between the feed 4 of the material to be ground and the region of the abrasive jet 10 or the use of a corresponding heating in the outer region of the feed 4 of the material to be ground. The source 12, or the particles of the material to be abraded, which in any case have been warmed, avoiding heat losses when entering the feed 4 of the material to be ground, for which purpose the feed tube 13 is insulated from the jacket 14 by temperature. surround. The heating source 11 or 12 (if used) can in principle be of any desired type and is therefore suitable for particular use for the intended purpose and according to market availability, so no further explanation of this point is required.

研磨噴射流或複數個研磨噴射流10之溫度就溫度而言特別有意義，且待研磨材料之溫度應至少大致對應於此研磨噴射流溫度。The temperature of the abrasive jet or plurality of abrasive jets 10 is particularly interesting in terms of temperature, and the temperature of the material to be abraded should at least substantially correspond to the temperature of the abrasive jet.

在操作條件下為氣體的任何物質或物質混合物可用於形成研磨噴射流10，其經由研磨噴射入口5引入研磨室3中。特別優先選擇使用空氣及/或氫氣及/或氬氣及/或惰性氣體，諸如氦氣及/或氮氣及/或所述操作介質之混合物。關於此點，應確保操作介質在各個研磨噴射入口5的入口噴嘴9之後的熱含量實質上不低於在此入口噴嘴9之前的熱含量。因為撞擊粉碎所必要之能量主要可利用流動能量，所以入口噴嘴9的入口15與其出口16之間的壓力降比較起來相當大(壓力能量以最大程度轉換成流動能量)，且溫度降也不是不重要。當有至少兩個研磨噴射流10彼此會合時或倍數的兩個研磨噴射流10時，此溫度降應特別藉由待研磨材料加熱至待研磨材料及研磨噴射流10在研磨室3的中心17區域內具有相同溫度的此一程度來補償。Any substance or mixture of substances that are gaseous under the operating conditions can be used to form the abrasive jet 10, which is introduced into the grinding chamber 3 via the abrasive jet inlet 5. Particular preference is given to using air and/or hydrogen and/or argon and/or inert gases, such as helium and/or nitrogen and/or mixtures of said operating medium. In this regard, it should be ensured that the heat content of the operating medium after the inlet nozzles 9 of the respective grinding jet inlets 5 is substantially not lower than the heat content before the inlet nozzles 9. Since the energy necessary for impact pulverization mainly utilizes the flow energy, the pressure drop between the inlet 15 of the inlet nozzle 9 and its outlet 16 is relatively large (pressure energy is converted to flow energy to the greatest extent), and the temperature drop is not important. When there are at least two abrasive jets 10 that meet each other or multiples of the two abrasive jets 10, this temperature drop should be heated, in particular, by the material to be ground to the material to be ground and the abrasive jet 10 in the center of the grinding chamber 3 This degree of the same temperature within the area is compensated.

設計及實行研磨噴射流10之製備方法為熟習本技藝者已知。Methods of making and implementing the abrasive jet 10 are well known to those skilled in the art.

在噴射研磨機1的本發明示例性具體例之圖像中，儲槽或產生裝置18(諸如槽18a)代表操作介質B的任何供應器，來自該槽的操作介質B係以引導裝置19的方式引導至研磨噴射入口5或複數個研磨噴射入口5，以形成研磨噴射流10或複數個研磨噴射流10。亦有可能使用例如壓縮機代替槽18a取得適當的操作介質B。然而，特別佳的是簡式鼓風機，最優先選擇為旋轉式鼓風機或徑向式風扇。In the image of an exemplary embodiment of the jet mill 1 of the present invention, a reservoir or generating device 18 (such as tank 18a) represents any supply of operating medium B from which operating medium B is directed The mode is directed to the abrasive jet inlet 5 or the plurality of abrasive jet inlets 5 to form a abrasive jet 10 or a plurality of abrasive jets 10. It is also possible to obtain a suitable operating medium B using, for example, a compressor instead of the groove 18a. However, it is particularly preferred to have a simple blower, the most preferred being a rotary blower or a radial fan.

特別以具備有此類型之空氣分級器7的噴射研磨機1為基準，在此有關的示例性具體例僅意欲示例，而非限制且應被如此了解，用於產生細粒子之製程係以具有整合之動態空氣分級器7的此噴射研磨機1進行。流體或氣體通常被用作為操作介質B，優先選擇為已述及之氫氣或氦氣或簡單的空氣。In particular, with reference to a jet mill 1 having an air classifier 7 of this type, the relevant exemplary embodiments are intended to be illustrative only, and are not limiting and should be so understood, the process for producing fine particles has This jet mill 1 of the integrated dynamic air classifier 7 is carried out. Fluid or gas is typically used as the operating medium B, preferably as hydrogen or helium or simple air as already mentioned.

此外，若分級轉子8具有固定或隨半徑減少(換言之，趨向其軸)而增加之淨高時，則有利且因此較佳的是流經的分級轉子8的表面積特別為固定的。另外或另一選擇地，可提供具有橫截面在流動方向上變寬的細料出口室。Furthermore, if the graded rotor 8 has a fixed or increased net height as the radius decreases (in other words, toward its axis), it is advantageous and therefore preferred that the surface area of the graded rotor 8 flowing therethrough is particularly fixed. Additionally or alternatively, a fines outlet chamber having a cross-section that widens in the direction of flow may be provided.

在噴射研磨機1的例子中，特別佳的改善在於分級轉子8具有可交換的共旋轉浸沒管20。A particularly preferred improvement in the example of jet mill 1 is that the staged rotor 8 has an exchangeable co-rotating immersion tube 20.

噴射研磨機1及其組份的示例性改善的更多細節及變型以參考圖2和圖3解釋於下。Further details and variations of the exemplary improvement of jet mill 1 and its components are explained below with reference to Figures 2 and 3.

可從圖2中之示意圖像觀察，噴射研磨機1包括整合之空氣分級器7，在噴射研磨機1經設計為例如流化床對向噴射研磨機或密相床噴射研磨機時，其為動態空氣分級器7，其有利地配置在噴射研磨機1的研磨室3中心。經研磨材料之標定細度可取決而研磨氣體的體積流量及分級器的旋轉速度而受到影響。As can be seen from the schematic image in Fig. 2, the jet mill 1 comprises an integrated air classifier 7, which is designed, for example, as a fluidized bed opposed jet mill or a dense bed jet mill, A dynamic air classifier 7, which is advantageously arranged in the center of the grinding chamber 3 of the jet mill 1. The nominal fineness of the ground material can be affected by the volumetric flow rate of the abrasive gas and the rotational speed of the classifier.

在根據圖2之噴射研磨機1的空氣分級器7之例子中，整個直立的空氣分級器7係以分級器容箱21圍住，該容箱實質上包含容箱上部件22及容箱下部件23。容箱上部件22及容箱下部件23的上緣及下緣分別各具備有向外引導之周圍凸緣24及25。兩個周圍凸緣24，25在空氣分級器8的安裝或功能狀態下相互平放且以適合的設施相互固定。適合於固定的設施為例如螺旋連接(未顯示)。鉗夾(未顯示)或類似物亦可充當為可鬆開之扣緊設施。In the example of the air classifier 7 of the jet mill 1 according to Fig. 2, the entire upright air classifier 7 is enclosed by a classifier tank 21 which substantially comprises the upper part 22 of the tank and the lower tank Component 23. The upper and lower edges of the upper casing member 22 and the lower casing member 23 are each provided with peripheral flanges 24 and 25 that are outwardly guided. The two surrounding flanges 24, 25 are placed one above the other in the installed or functional state of the air classifier 8 and are secured to one another by suitable means. Suitable facilities for attachment are, for example, screw connections (not shown). A clamp (not shown) or the like can also act as a releasable fastening device.

在凸緣周圍的實際上任何所欲位置上，兩個周圍凸緣24及25係以活節接頭26在鬆開凸緣連接設施之後使得容箱上部件22可以與容箱下部件23有關的箭號27方向向上轉動且容箱上部件22可自下方通達及容箱下部件23可從上方通達的此一方式彼此連接。容箱下部件23就其部件而言為兩個部件形式，且實質上包含在其上開口端具有周圍凸緣25之圓筒狀分級室容箱28及以圓錐形式向下漸縮之排放錐體29。排放錐體29及分級室容箱28互相平放在具有凸緣30，31的上端及下端，且排放錐體29及分級室容箱28的兩個凸緣30，31與周圍凸緣24，25相同的方式以可鬆開之扣緊設施(未顯示)彼此連接。依此方式組裝之分級器容箱21懸掛在支撐臂28a中或支撐臂28a上，許多支撐臂以儘可能均勻的分開間隔分布在噴射研磨機1之空氣分級器7的分級器或壓縮器容箱21周圍，且在圓筒狀分級室容箱28上起作用。In virtually any desired position around the flange, the two peripheral flanges 24 and 25 are such that the joint member 26 can be associated with the lower box member 23 after the flange joint is loosened by the joint joint 26 The arrow 27 is rotated upwardly and the upper container member 22 is accessible from below and the container lower member 23 is accessible from above in this manner. The lower container part 23 is in the form of two parts in terms of its components, and substantially comprises a cylindrical grading chamber tank 28 having a peripheral flange 25 at its upper open end and a discharge cone which tapers downwardly in the form of a cone Body 29. The discharge cone 29 and the classification chamber tank 28 are placed flush with each other at the upper and lower ends of the flanges 30, 31, and the discharge cone 29 and the two flanges 30, 31 of the classification chamber tank 28 and the surrounding flange 24, 25 The same way is connected to each other with a releasable fastening device (not shown). The classifier tank 21 assembled in this manner is suspended in the support arm 28a or on the support arm 28a, and the plurality of support arms are distributed at a uniform interval as evenly as possible in the classifier or compressor capacity of the air classifier 7 of the jet mill 1. Around the tank 21, it acts on the cylindrical grading chamber tank 28.

空氣分級器7的內部容箱組件之另一重要部件為分級輪8，其具有上蓋板32、在遠離該上蓋板的軸之外流側上的下蓋板33及具有適宜輪廓之葉片34，該葉片係配置在兩個蓋板32與33的外緣之間，牢固地連接至該蓋板且均勻地分布於分級輪8周邊。在此空氣分級器7的例子中，分級輪8的驅動係以上蓋板32的方式提供，而下蓋板33為外流側上的蓋板。分級輪8的架設包含適宜地正向驅動之分級輪軸35，其上端係以分級器容箱21引出及下端支撐在分級器容箱21內以懸吊軸承不可旋轉之分級輪8。自分級器容箱21引出分級輪軸35係發生在一對機製板36，37中，該機製板在頂端呈截錐形式之容箱末端部位38的上端封閉分級器容箱21，導引分級輪軸35且密封此軸通道而不阻礙分級輪軸35的旋轉移動。可將上板36適宜地指配為對分級輪軸35不可旋轉的凸緣且以旋轉軸承35a的方式不可旋轉地支撐在下板37上，將下板就其部件而指配至容箱末端部位38。在外流側上的蓋板33底側平放在周圍凸緣24與25之間的共同平面上，使得分級輪8以其整體配置在絞接之容箱上部件22內。在圓錐形末端部位38區域中，容箱上部件22亦具有待研磨材料之進料4的管狀產物進料通孔39，該通孔的縱軸與分級輪8的旋轉軸40及其驅動或分級輪軸35平行延伸，且該通孔徑向配置在容箱上部件22的外側上，儘可能遠離分級輪8的此旋轉軸40及其驅動或分級輪軸35。Another important component of the internal container assembly of the air classifier 7 is a grading wheel 8 having an upper cover 32, a lower cover 33 on the flow side away from the shaft of the upper cover, and a blade 34 having a suitable profile. The blade is disposed between the outer edges of the two cover plates 32 and 33, is firmly connected to the cover plate and is evenly distributed around the periphery of the classifying wheel 8. In the example of the air classifier 7, the drive of the classifying wheel 8 is provided in the manner of the upper cover 32, and the lower cover 33 is the cover on the outflow side. The grading of the grading wheel 8 includes a grading wheel shaft 35 that is suitably driven in the forward direction, the upper end of which is led by the classifier tank 21 and the lower end of which is supported in the classifier tank 21 to suspend the grading wheel 8 which is non-rotatable. The grading wheel axle 35 from the classifier tank 21 takes place in a pair of mechanism plates 36, 37 which close the classifier tank 21 at the upper end of the truncated cone end portion 38 of the container at the top end, guiding the grading wheel axle 35 and sealing the shaft passage without obstructing the rotational movement of the stepping wheel shaft 35. The upper plate 36 can be suitably assigned as a flange that is non-rotatable to the stepped axle 35 and non-rotatably supported on the lower plate 37 in the manner of a rotary bearing 35a, the lower plate being assigned to the container end portion 38 for its components. . The bottom side of the cover 33 on the outflow side lies flat on a common plane between the peripheral flanges 24 and 25 such that the grading wheel 8 is integrally disposed within the spliced upper box member 22. In the region of the conical end portion 38, the upper container part 22 also has a tubular product feed through opening 39 for the feed 4 of the material to be ground, the longitudinal axis of the through hole and the axis of rotation 40 of the classifying wheel 8 and its drive or The grading axles 35 extend in parallel and are arranged radially on the outside of the upper part 22 of the tank, as far as possible from this rotating shaft 40 of the grading wheel 8 and its drive or grading axle 35.

分級器容箱21接納管狀出口通孔20，其與分級輪8共軸配置且以上末端正好平放在外流側上的蓋板33之下，但未與其連接。以共軸佈置在出口通孔20的下端而形成為管的是出口室41，其同樣為管狀，但是其直徑遠比出口通孔20的直徑更大，且在本發明之示例性具體例的例子中為至少兩倍的出口通孔20直徑。在出口通孔20與出口室41之間的過渡區因此有顯著的直徑改變。出口通孔20係***出口室41的上蓋板42內。在出口室41的底部以可拆卸蓋43封閉。包含出口通孔20及出口室41之組合件以許多支撐臂44頂住，該等支撐臂係以似星狀方式均勻地分布在組合件周圍，以其內端牢固地連接至出口通孔20區域內的組合件，且其外端牢固至分級器容箱21。The classifier tank 21 receives a tubular outlet through hole 20 that is coaxially disposed with the classifying wheel 8 and that has the upper end just below the cover plate 33 on the outflow side but is not connected thereto. Formed as a tube coaxially disposed at the lower end of the outlet through hole 20 is an outlet chamber 41 which is also tubular but has a diameter that is much larger than the diameter of the outlet through hole 20, and is exemplified in an exemplary embodiment of the present invention. In the example, it is at least twice the diameter of the outlet through hole 20. The transition between the outlet through hole 20 and the outlet chamber 41 thus has a significant diameter change. The outlet through hole 20 is inserted into the upper cover 42 of the outlet chamber 41. At the bottom of the outlet chamber 41 is closed with a detachable cover 43. The assembly including the outlet through-hole 20 and the outlet chamber 41 is supported by a plurality of support arms 44 that are evenly distributed around the assembly in a star-like manner with their inner ends firmly connected to the outlet through-holes 20 The assembly within the area with its outer end secured to the classifier housing 21.

出口通孔20以圓錐形環狀容箱45包圍，其下方較大的外徑至少大致對應於出口室41的直徑，且其上方較小的外徑至少大致對應於分級輪8的直徑。支撐臂44終止在環狀容箱45的圓錐形壁且牢固地連接至此壁，此壁就其部件而言亦為包含出口通孔20及出口室41之組合件的一部分。The outlet through hole 20 is surrounded by a conical annular tank 45 having a larger outer diameter at least substantially corresponding to the diameter of the outlet chamber 41 and a smaller outer diameter at least substantially corresponding to the diameter of the classifying wheel 8. The support arm 44 terminates in a conical wall of the annular tank 45 and is securely attached to the wall, which wall is also part of the assembly comprising the outlet through bore 20 and the outlet chamber 41 for its components.

支撐臂44及環狀容箱45為沖洗空氣裝置(未顯示)之部件，沖洗空氣防止材料自分級器容箱21內部穿透至介於分級輪8或更精確為其下蓋板3與出口通孔20之間的間隙內。為了容許此沖洗空氣進入環狀容箱45中且從此前進至保持暢通的間隙，故使支撐臂44形成為管形，以其外端部位引導通過分級器容箱21壁且以進氣過濾器46的方式連接至沖洗空氣源(未顯示)。將環狀容箱45在頂端以多孔板47封閉，且間隙本身可以多孔板47與分級輪8的下蓋板33之間的區域內以軸調整之環狀盤調整。The support arm 44 and the annular container 45 are components of a flushing air device (not shown) that prevents material from penetrating from inside the classifier housing 21 to the leveling wheel 8 or more precisely to its lower cover 3 and outlet Within the gap between the through holes 20. In order to allow this flushing air to enter the annular tank 45 and proceed therefrom to maintain a clear gap, the support arm 44 is formed into a tubular shape with its outer end portion guided through the wall of the classifier tank 21 and with an air intake filter The way 46 is connected to the flushing air source (not shown). The annular tank 45 is closed at the top end with a perforated plate 47, and the gap itself can be adjusted in an axially adjustable annular disk in the region between the perforated plate 47 and the lower cover 33 of the classifying wheel 8.

出口室41的出口係由細料排放管48所形成，其係自外部引導至分級器容箱21中且以切線方式連接至出口室41。細料排放管48為產物出口6的組件。偏向錐體49用以包覆細料排放管48至出口室41的入口。The outlet of the outlet chamber 41 is formed by a fines discharge pipe 48 that is externally guided into the classifier tank 21 and connected to the outlet chamber 41 in a tangential manner. The fines discharge pipe 48 is an assembly of the product outlet 6. The deflecting cone 49 is used to cover the inlet of the fine material discharge pipe 48 to the outlet chamber 41.

在圓錐形容箱末端部位38的下端，分級空氣入口螺旋50及粗粒材料排放51經指配與容箱末端部位38呈水平配置。分級空氣入口螺旋50的旋轉方向與分級輪8的旋轉方向相反。當空氣分級器7準備操作時，粗粒材料排放51可拆卸地指配至容箱末端部位38，容箱末端部位38的下端指配凸緣52且粗粒材料排放51的上端指配凸緣53，且兩個凸緣52及53以已知的設施彼此以可鬆開方式連接。At the lower end of the conical tank end portion 38, the graded air inlet helix 50 and the coarse material discharge 51 are assigned to be horizontally disposed with the tank end portion 38. The direction of rotation of the stepped air inlet helix 50 is opposite to the direction of rotation of the stepping wheel 8. When the air classifier 7 is ready for operation, the coarse material discharge 51 is detachably assigned to the tank end portion 38, the lower end of the tank end portion 38 is assigned the flange 52 and the upper end of the coarse material discharge 51 is assigned a flange 53. The two flanges 52 and 53 are releasably connected to one another in a known arrangement.

經設計之分散區以54表示。在內緣上經機械加工(成斜面)以產生平滑流動及單純內襯的凸緣以55表示。The designed dispersion zone is indicated at 54. A flange that is machined (beveled) on the inner edge to create a smooth flow and simple lining is indicated at 55.

最後，可交換之保護管56亦佈置在出口通孔20的內壁上作為閉合部件，且對應之保護管57可佈置在出口室41的內壁上。Finally, the exchangeable protective tube 56 is also disposed on the inner wall of the outlet through hole 20 as a closing member, and the corresponding protective tube 57 can be disposed on the inner wall of the outlet chamber 41.

在分級器7在所示之操作狀態下開始操作時，將分級空氣在壓力梯度下及以根據目的所選擇之進入速度以分級空氣入口螺旋50的方式引入空氣分級器7內。由於分級空氣係利用特別與容箱末端部位38的圓錐度組合的螺旋引入，使得分級空氣以螺旋向上升高至分級輪8區域內。同時，包含不同質量之固體粒子的〝產物〞係以產物進料通孔39的方式引入分級器容箱21內。將此產物中的粗粒材料(亦即較大質量的粒子部分)與分級空氣相反前進至粗粒材料排放51區域中且可用於進一步處理。將細料(亦即較小質量的粒子部分)與分級空氣混合，從外部向內徑向經過分級輪8前進至出口通孔20中，前進至出口室41中且最後以細料出口管48的方式前進至細料出口58中，且從此處前進至其中操作介質呈流體形式(諸如空氣)的過濾器中及將細料彼此分離。細料的粗粒成分係以離心力從分級輪8徑向移出且與粗粒材料混合，以分級器容箱21留下粗粒材料或持續在分級器容箱21中循環，直到變成具有使其以分級空氣排放的此一粒子大小的細料為止。When the classifier 7 begins operation in the illustrated operational state, the staged air is introduced into the air classifier 7 in a manner of a stepped air inlet helix 50 under a pressure gradient and at an entry speed selected according to the purpose. Since the graded air system is introduced by a helix, which is particularly combined with the conicality of the tank end portion 38, the graded air is raised in a spiral upward into the region of the classifier wheel 8. At the same time, the lanthanum product lanthanum containing solid particles of different qualities is introduced into the classifier tank 21 in the manner of the product feed through-holes 39. The coarse particulate material (i.e., the larger mass fraction of particles) in this product is advanced in tandem with the graded air into the coarse particulate material discharge 51 region and is available for further processing. The fines (i.e., the smaller mass fractions) are mixed with the staged air, advanced radially inwardly from the outside through the grading wheel 8 into the outlet passage 20, advanced into the outlet chamber 41 and finally with the fines outlet tube 48. The way proceeds to the fines outlet 58 and from there proceeds to a filter in which the operating medium is in a fluid form, such as air, and separates the fines from one another. The coarse fraction of the fine material is radially removed from the classifying wheel 8 by centrifugal force and mixed with the coarse material, leaving the coarse material in the classifier tank 21 or continuously circulating in the classifier tank 21 until it becomes This particle-sized fine material is discharged by the classified air.

由於從出口通孔20至出口室41的橫截面突然變寬，使得於此發生顯著減低的細料-空氣混合物流速。此混合物因此以極低的流速以細料出口管48的方式經過出口室41進入細料出口58中，且在出口室41壁上只產生少量磨耗物質。就此理由而言，保護管57亦僅為高預先警戒措施。然而，就獲得好的分離技術的理由而言，在分級輪8中的高流速仍普遍於排放或出口通孔20中，就此理由而言，保護管56比保護管57更重要。特別重要的是直徑隨著從出口通孔20進入出口室41的過渡區之直徑變寬而改變。Due to the sudden widening of the cross section from the outlet through hole 20 to the outlet chamber 41, a significantly reduced fines-air mixture flow rate occurs. This mixture thus enters the fines outlet 58 through the outlet chamber 41 at a very low flow rate in the form of a fines outlet tube 48, and produces only a small amount of abrasive material on the wall of the outlet chamber 41. For this reason, the protective tube 57 is also only a high pre-warning measure. However, for reasons of good separation techniques, the high flow rate in the classifying wheel 8 is still common in the discharge or outlet through-holes 20, for which reason the protective tube 56 is more important than the protective tube 57. It is particularly important that the diameter changes as the diameter of the transition zone from the outlet through-hole 20 into the outlet chamber 41 becomes wider.

而且，由於以所述方式細分分級器容箱21及指配分級器組件至個別部件容箱，使得空氣分級器7可依次完整保養且有受損組件可在相當少的工作量下及短的保養時間內更換。Moreover, since the classifier tank 21 and the indexing classifier assembly are subdivided into individual component tanks in the manner described, the air classifier 7 can be fully maintained in sequence and the damaged components can be operated at a relatively small amount and with a small amount of work. Replace during maintenance time.

在圖2的示意圖像中，雖然具有兩個蓋板32和33及配置在其間且具有葉片34的葉片環59之分級輪8仍以已知具有為平行且有平行表面的蓋板32和33之慣常形式表現，但是在圖3中表現有利發展的空氣分級器7之進一步示例性具體例的分級輪8。In the schematic image of Fig. 2, although the grading wheel 8 having the two cover plates 32 and 33 and the blade ring 59 disposed therebetween and having the vanes 34 still has the cover plates 32 and 33 which are known to have parallel and parallel surfaces. The usual form of performance, but in FIG. 3, a grading wheel 8 of a further exemplary embodiment of an advantageous air classifier 7 is shown.

根據圖3的此分級輪8除了具有葉片34的葉片環59以外尚包括上蓋板32和在遠離該上蓋板的軸之外流側上的下蓋板33，且可在旋轉軸40周圍旋轉，因而在空氣分級器7的縱軸周圍旋轉。分級輪8的直徑維度垂直於旋轉軸40，亦即垂直於空氣分級器7的縱軸，與旋轉軸40及因而該縱軸是否為垂直或水平無關。在外流側上的下蓋板33同心地圍住出口通孔20。葉片34連接至該兩個蓋板33和32。於是不同於先前技藝的兩個蓋板32和33經形成為圓錐形，較佳地係以上蓋板32與外流側上的蓋板33之距離變得大於與葉片34之環59向內(亦即趨向旋轉軸40)的距離之方式精確形成，且優先選擇以連續形成，諸如以線性或非線性，且更優先選擇使得流經的圓筒套表面積就葉片出口邊緣與出口通孔20之間的每個半徑而言保持不變。在已知解法的例子中，外流速度係由於半徑變得較小而變得較慢，在此解法的例子中保持不變。The grading wheel 8 according to FIG. 3 comprises, in addition to the blade ring 59 of the blade 34, an upper cover plate 32 and a lower cover plate 33 on the flow side outside the shaft remote from the upper cover plate, and is rotatable around the rotary shaft 40. Thus, it rotates around the longitudinal axis of the air classifier 7. The diameter dimension of the classifying wheel 8 is perpendicular to the axis of rotation 40, i.e. perpendicular to the longitudinal axis of the air classifier 7, independent of whether the axis of rotation 40 and thus the axis is vertical or horizontal. The lower cover 33 on the outflow side concentrically surrounds the outlet through hole 20. The vanes 34 are connected to the two cover plates 33 and 32. Thus, the two cover plates 32 and 33 different from the prior art are formed into a conical shape, preferably the distance between the upper cover plate 32 and the cover plate 33 on the outflow side becomes greater than the ring 59 of the blade 34 (also That is, the manner of the distance toward the rotating shaft 40) is precisely formed, and is preferably selected to be continuously formed, such as linear or non-linear, and more preferably such that the surface area of the cylindrical sleeve flowing therethrough is between the blade outlet edge and the outlet through hole 20. It remains the same for each radius. In the example of the known solution, the outflow velocity becomes slower due to the smaller radius, which remains unchanged in the example of this solution.

除了上述及圖3中所解釋之上蓋板32和下蓋板33的設計變型以外，亦有可能僅以該兩個蓋板32或33中之一以所解釋之方式形成為圓錐形，而另一個蓋板33或32為平面形，如與根據圖2之示例性具體例有關的兩個蓋板32及33之例子。具有非平行表面的蓋板形狀特別在此例子中至少可大致使得流經的圓筒套表面積就葉片出口邊緣與出口通孔20之間的每個半徑而言保持不變。In addition to the design variants of the upper cover 32 and the lower cover 33 explained above and illustrated in FIG. 3, it is also possible to form the conical shape only in one of the two cover plates 32 or 33 in the manner explained. The other cover plate 33 or 32 is planar, as is the case with the two cover plates 32 and 33 associated with the exemplary embodiment of FIG. The shape of the cover plate having non-parallel surfaces, in particular in this example, can at least substantially maintain the surface area of the sleeve that flows through as a function of each radius between the exit edge of the blade and the exit through-hole 20.

在根據本發明之製程的特定具體例中，在研磨期間添加表面改質劑。在根據本發明之製程中的表面改質特別有效，因為當粒子在研磨機內部相撞時，從經研磨之細粒子形成混濁材料且可將表面改質劑引入此混濁材料中，可特別優先選擇噴霧至該材料中。結果，表面改質劑在結合反應期間不與研磨機壁接觸，所以防止結塊。此結塊象徵機械或分級機械研磨機有大的缺點及大的問題。表面改質劑優先選擇利用噴嘴引入，優先選擇為雙流體噴嘴，有可能使介質霧化成與研磨氣體相同的介質。較佳的是該改質劑係經由噴嘴注入研磨區內，特別優先選擇在與研磨噴嘴相同的高度下。In a particular embodiment of the process according to the invention, a surface modifying agent is added during the grinding. Surface modification in the process according to the present invention is particularly effective because it is particularly preferred to form a turbid material from the ground fine particles and to introduce a surface modifying agent into the turbid material when the particles collide inside the grinder. Spray is selected into the material. As a result, the surface modifier does not come into contact with the wall of the grinder during the bonding reaction, thus preventing agglomeration. This agglomeration symbolizes the major drawbacks and major problems of mechanical or graded mechanical grinders. The surface modifier is preferably introduced by means of a nozzle, preferably a two-fluid nozzle, which makes it possible to atomize the medium into the same medium as the grinding gas. Preferably, the modifier is injected into the grinding zone via a nozzle, particularly preferably at the same height as the grinding nozzle.

此類型之表面改質的一項特別優勢在於事實是由於研磨而使活性/新鮮表面實際上得以當場塗佈/摻雜。此增加待研磨材料的表面與塗料/摻雜劑的交互作用且尤其導致更強的結合。進一步的優勢可為經研磨材料的穩定(例如，關於再黏聚)可由於研磨期間的同步塗佈/摻雜而達成。A particular advantage of this type of surface modification is the fact that the active/fresh surface is actually coated/doped on the spot due to grinding. This increases the interaction of the surface of the material to be abraded with the coating/dopant and in particular leads to a stronger bond. A further advantage may be that the stabilization of the ground material (eg, with respect to re-gluing) may be achieved due to simultaneous coating/doping during grinding.

原則上，在研磨條件下可以液體、溶液或熔融流噴霧至研磨室中的所有表面改質劑皆可用於根據本發明之製程中。在本發明的範圍內較佳的表面改質劑為矽酸鈉、鹼(例如，NaOH及KOH)、酸(例如，硫酸、氫氯酸、硝酸)、有機矽化合物(例如，改質或未改質之矽烷、聚矽氧烷、有機改質之聚矽氧烷、矽油、聚矽氧聚醚丙酸酯)、有機聚合物、丙烯酸酯、聚乙烯醇(PVA)、蠟(例如，聚乙烯蠟)及金屬鹽(摻雜)。雖然不是全部，但是此等表面改質劑的一些實例在WO 2004/055120、WO 2004/055105、WO 2004/054927或EP 1477457中提出。將該等文件的內容藉此明確地包括於本發明的主題中。In principle, all surface modifying agents which can be sprayed into the grinding chamber in a liquid, solution or melt stream under milling conditions can be used in the process according to the invention. Preferred surface modifying agents within the scope of the present invention are sodium citrate, bases (e.g., NaOH and KOH), acids (e.g., sulfuric acid, hydrochloric acid, nitric acid), organic hydrazine compounds (e.g., modified or not). Modified decane, polyoxyalkylene, organically modified polyoxyalkylene, eucalyptus oil, polyoxyl polyether propionate), organic polymer, acrylate, polyvinyl alcohol (PVA), wax (eg, poly Vinyl wax) and metal salt (doped). Although not all, some examples of such surface modifiers are set forth in WO 2004/055120, WO 2004/055105, WO 2004/054927 or EP 1477457. The contents of such documents are hereby expressly included in the subject matter of the present invention.

表面覆蓋特別有利地以聚矽氧聚醚丙酸酯聚合物執行，其係以例如為名稱銷售。特別優先選擇該等為聚矽氧聚醚丙酸酯聚合物或聚矽氧聚醚甲基丙酸酯聚合物，諸如那些在EP 0999230 A1中所述者，而最特別優先選擇為對應於EP 099230 A1之具有從1至50重量%之聚醚過量的聚合物，優先選擇為5至30重量%，特別優先選擇為10至20重量%。將此特許公開之專利申請案的主題藉此明確地包括於本發明的主題中。The surface covering is particularly advantageously carried out with a polyoxyl polyether propionate polymer, for example Sold for the name. It is particularly preferred that these are polyoxyl polyether propionate polymers or polyoxyl polyether methyl propionate polymers, such as those described in EP 0999230 A1, with the most particular preference being corresponding to EP. 099230 A1 has a polyether excess polymer of from 1 to 50% by weight, preferably from 5 to 30% by weight, particularly preferably from 10 to 20% by weight. The subject matter of this copending patent application is hereby expressly incorporated in the subject matter of the present invention.

在本發明的範圍內，最特別優先選擇非晶形SiO₂ (特別為沉澱矽石)、矽酸鹽(例如，鋁矽酸鹽)、電弧矽石、熱解矽石、半凝膠或矽膠之固體在根據本發明之製程的此變型中研磨且以聚矽氧聚醚丙酸酯、聚乙烯醇(PVA)、丙酸酯、蠟及金屬鹽塗佈或摻雜。塗料或摻雜劑與待研磨材料的此組合特別佳，因為在習知的製程中迄今仍有必要先執行塗佈或摻雜及接著在機械或分級機械研磨機中研磨。此新式製程第一次將塗佈或摻雜及研磨成功組合在一個步驟中且還是達成經研磨材料至少等於及甚至常比以機械或分級機械研磨機更卓越的粒度分布。與習知的製程比較，此材料組合一方面消除在製程中的步驟，但另一方面亦達成卓越的產品，因為根據本發明之製程導致在粒度分布中較低比例之細料含量且有可能完全塗佈/摻雜待研磨材料的表面。Within the scope of the invention, amorphous SiO ₂ (especially precipitated vermiculite), citrate (for example aluminosilicate), arc vermiculite, pyrolytic vermiculite, semi-gel or silicone are preferred. The solid is ground in this variant of the process according to the invention and coated or doped with polyoxyl polyether propionate, polyvinyl alcohol (PVA), propionate, wax and metal salt. This combination of coating or dopant with the material to be abraded is particularly preferred since it has heretofore been necessary in prior art processes to perform coating or doping and then to grind in a mechanical or fractional mechanical mill. This new process combines coating or doping and grinding successfully in one step for the first time and still achieves a particle size distribution that is at least equal to and even often superior to mechanical or fractional mechanical mills. In contrast to conventional processes, this combination of materials eliminates the steps in the process on the one hand, but also achieves a superior product on the other hand, since the process according to the invention results in a lower proportion of fines content in the particle size distribution and is possible The surface of the material to be abraded is completely coated/doped.

原則上，雖然所有的有機及無機固體皆可根據本發明之製程研磨，但是此製程就元素週期表的第三及第四主族之金屬的非晶形氧化物提供特別的優勢。此適用於凝膠及具有不同的結構種類之非晶形固體。以沉澱矽石、熱解矽石、電弧矽石、矽酸鹽、半凝膠及矽膠特別佳，矽膠不僅包含水凝膠，亦包含氣凝膠及乾凝膠。該等材料常被用於例如作為漆料中的消光劑之應用中，在此精確限定之粒度分布具重要性，而且例如太高的細料含量是有害的，因為增稠性質由此受到損害。除了特定的粒度分布以外，以雜質(諸如鐵)的低污染在許多應用中非常有利。根據本發明之製程第一次以特定的粒度分布與非常低的外來元素污染之組合成功產製元素週期表的第三及第四主族之金屬的非晶形氧化物，特別為二氧化矽。In principle, although all organic and inorganic solids can be milled according to the process of the present invention, this process provides particular advantages with regard to the amorphous oxide of the metals of the third and fourth main groups of the Periodic Table of the Elements. This applies to gels and amorphous solids with different structural types. It is particularly good for precipitating vermiculite, pyrolytic vermiculite, arc vermiculite, citrate, semi-gel and silicone. The silicone contains not only hydrogels but also aerogels and xerogels. Such materials are often used, for example, in the application as a matting agent in paints, where the precisely defined particle size distribution is of importance and, for example, too high a fines content is detrimental because the thickening properties are thereby impaired . In addition to the specific particle size distribution, low contamination with impurities such as iron is very advantageous in many applications. The process according to the present invention, for the first time, successfully produces amorphous oxides of metals of the third and fourth main groups of the Periodic Table of the Elements, in particular cerium oxide, in a combination of a specific particle size distribution and very low foreign elemental contamination.

測量方法Measurement methods 利用雷射繞射測定粒子大小Measuring particle size using laser diffraction

用於測定粉狀固體之粒子大小分布的雷射繞射係以粒子取決於其大小而散射或繞射在所有方向上具有不同強度型式的單色雷射束之光的現象為基準。以雷射束照射之粒子直徑越小，則單色雷射束之散射或繞射角度越大。The laser diffraction system for determining the particle size distribution of the powdery solid is based on the phenomenon that the particles scatter or diffract light of a monochromatic laser beam having different intensity patterns in all directions depending on the size thereof. The smaller the particle diameter of the laser beam, the larger the scattering or diffraction angle of the monochromatic laser beam.

進行測量的以下方式係以沉澱矽石樣品為基準說明。在親水性沉澱矽石的例子中，樣品製備及測量係以完全去離子水作為分散流體來執行，而在以水不可適當地弄濕沉澱矽石的例子中使用純乙醇。在開始測量之前，先允許LS 230雷射繞射粒子大小分析儀(來自Beckman Coulter；測量範圍：0.04-2000微米)及流體模組(Small Volume Module Plus，120毫升，來自Beckman Coulter)溫熱2小時，且將模組以完全去離子水沖洗三次。用於測量疏水性沉澱矽石的沖洗操作係以純乙醇進行。The following methods for performing the measurement are based on the precipitation of the vermiculite sample. In the example of the hydrophilic precipitated vermiculite, sample preparation and measurement are performed with completely deionized water as a dispersion fluid, and pure ethanol is used in the example where water is not suitable for wetting the precipitated vermiculite. Allow the LS 230 laser diffraction particle size analyzer (from Beckman Coulter; measuring range: 0.04-2000 μm) and the fluid module (Small Volume Module Plus, 120 ml from Beckman Coulter) to warm before starting the measurement. Hours and the module was rinsed three times with fully deionized water. The flushing operation for measuring hydrophobic precipitated vermiculite is carried out in pure ethanol.

在LS 230雷射繞射粒子大小分析儀的分析儀軟體中，與以Mie原理為基準評估有關的以下光學參數(儲存於.rfd檔中)：In the analyzer software of the LS 230 Laser Diffraction Particle Size Analyzer, the following optical parameters (stored in the .rfd file) related to the evaluation based on the Mie principle are:

分散流體的折射率D. I.實數_水 =1.332(乙醇為1.359)；固體(樣品材料)的折射率實數_矽石 =1.46The refractive index of the dispersed fluid is DI real _water = 1.332 (ethanol is 1.359); the refractive index of the solid (sample material) is real number _meteorite = 1.46

虛數=0.1Imaginary number = 0.1

形狀因子=1Shape factor=1

此外，應該設定與粒子測量有關的以下參數：In addition, the following parameters related to particle measurement should be set:

測量時間=60秒Measurement time = 60 seconds

測量次數=1Number of measurements = 1

泵送速度=75%Pumping speed = 75%

取決於樣品本性而定，可利用刮勺以粉狀固體直接引入，或利用2毫升可棄式吸管以懸浮形式引入分析儀的流模組(Small Volume Module Plus)中。當達到測量所需之樣品濃度時(最優光學遮蔽)，則LS 230雷射繞射粒子大小分析儀的軟體顯示〝OK〞。經研磨之沉澱矽石係藉由暴露於超聲波60秒而分散於流體模組中，該分散係利用來自Sonics之Vibra Cell VCX 130，具有CV 181超聲波轉化器及6毫米超聲波尖端，以70%振幅且同時泵送循環。在未經研磨之沉澱矽石的例子中，分散係藉由在流體模組中泵送循環60秒來執行，而不暴露於超聲波。測量係在室溫下執行。分析儀軟體係以Mie原理為基準且輔以先前建立之光學參數(.rfd檔)從原始數據計算粒子大小的體積分布及d50值(中間值)。Depending on the nature of the sample, it can be introduced directly into the powdered solids using a spatula or in a suspended form into a flow module (Small Volume Module Plus) using a 2 ml disposable pipette. When the sample concentration required for the measurement is reached (optimal optical masking), the software of the LS 230 laser diffraction particle size analyzer displays 〝OK〞. The ground precipitated vermiculite was dispersed in a fluid module by exposure to ultrasonic waves for 60 seconds using a Vibra Cell VCX 130 from Sonics with a CV 181 ultrasonic transducer and a 6 mm ultrasonic tip with 70% amplitude At the same time, the pumping cycle. In the case of unground precipitated vermiculite, the dispersion is performed by pumping a cycle for 60 seconds in the fluid module without exposure to ultrasonic waves. The measurement system was performed at room temperature. The analyzer soft system calculates the particle size distribution and the d50 value (intermediate value) from the raw data based on the Mie principle and supplemented by previously established optical parameters (.rfd file).

ISO 13320〝粒子大小分析-雷射繞射方法指南〞詳細說明用於測定粒子大小分布的雷射繞射方法。熟習本技藝者找得到與以Mie原理為基準之評估有關的常使用之固體及分散流體的光學參數之名冊。ISO 13320 〝 Particle Size Analysis - Guide to Laser Diffraction Methods 〞 Detailed description of laser diffraction methods for determining particle size distribution. Those skilled in the art will be able to find a list of optical parameters of commonly used solid and dispersed fluids related to the evaluation based on the Mie principle.

僅以實例方式使本發明以示例性具體例為基準呈現於說明中及表現於圖式中，且不受限於該等說明及圖式，但反而包含由熟習本技藝者可從本發明文件，特別在申請專利範圍及在此說明的介紹部分中的概括圖像範圍內，以及示例性具體例的說明及其在圖式中的圖像可取得且組合其專業知識及先前技藝的所有變化、修改、取代及組合。可特別將所有的個別特色及提昇本發明的可能性與實施本發明的各種方式組合。The present invention has been shown by way of example only and by way of example only, and is not limited by the description and drawings, but rather by those skilled in the art In particular, within the scope of the generalized image in the scope of the patent application and the description section described herein, as well as the description of the exemplary embodiments and the images in the drawings, all the changes in the expertise and prior art can be obtained. , modification, substitution and combination. All of the individual features and possibilities for enhancing the invention may be combined with various ways of practicing the invention.

實例1：Example 1:

將來自Evonik Degussa GmbH之HK 400在來自Hosokawa Alpine AG之AFG 200 Aeroplex流化床對向噴射研磨機中在76℃之研磨空氣入口溫度(研磨室內部溫度=60℃)及0.4巴之壓力(絕對)下研磨且以Rad 2300聚矽氧聚醚丙烯酸酯覆蓋。此包含將塗料以位於與研磨噴嘴相同平面上的雙流體噴嘴(未描述於圖1至3中)(三個研磨噴嘴以120°間隔分開，而雙流體噴嘴係在該等之間的60°處)的方式注入至研磨機中。饋入7.4質量%之Rad 2300(Rad 2300具有約43.9重量%之碳含量)。在最終產物中測得3.2重量%之碳含量，亦即考慮到Rad 2300的碳含量，多少有些定量覆蓋達成而沒有聚醚損失。以濕式塗佈及添加相同百分比的Rad 2300僅在最終產物中測得介於2.5與2.8重量%之間的碳。Will come from Evonik Degussa GmbH HK 400 was ground in an AFG 200 Aeroplex fluidized bed counter jet mill from Hosokawa Alpine AG at a grinding air inlet temperature of 76 ° C (grinding room temperature = 60 ° C) and a pressure of 0.4 bar (absolute) Rad 2300 polyoxyl polyacrylate acrylate overlay. This involves placing the coating in a two-fluid nozzle (not depicted in Figures 1 to 3) on the same plane as the grinding nozzle (three grinding nozzles are separated by 120°, and the two-fluid nozzle is 60° between the two) The way to be injected into the grinder. Feeding 7.4% by mass Rad 2300 ( Rad 2300 has a carbon content of about 43.9 wt%). A carbon content of 3.2% by weight was measured in the final product, that is, Rad 2300's carbon content, some quantitative coverage is achieved without loss of polyether. Wet coating and adding the same percentage Rad 2300 measured between 2.5 and 2.8% by weight of carbon only in the final product.

因此，在濕式塗佈的例子中，大量的表面改質劑不在矽石上，而是以水洗出。此顯示根據本發明之製程在以具有水溶性部分的表面改質劑覆蓋載體材料。產物具有4.7微米之d₅₀ 值。Therefore, in the example of wet coating, a large amount of the surface modifier is not on the vermiculite, but is washed out with water. This shows that the process according to the invention covers the carrier material with a surface modifying agent having a water soluble portion. The product having the d ₅₀ value of 4.7 microns.

實例2：Example 2:

將來自Evonik Degussa GmbH之50在來自Netzsch-Condux之CGS 50型流化床對向噴射研磨機在80℃之研磨空氣溫度及0.36巴之壓力(絕對)下以來自Deurex 之PE蠟(熔點範圍：98-103℃)覆蓋。塗佈係以類似於實例1的方式執行。產物具有5.8微米之d₅₀ 值。Will come from Evonik Degussa GmbH 50 covered with a PE wax from Deurex (melting point range: 98-103 ° C) at a CGS 50 fluidized bed counter jet mill from Netzsch-Condux at a grinding air temperature of 80 ° C and a pressure (absolute) of 0.36 bar (absolute) . The coating system was carried out in a manner similar to that of Example 1. The product having the d ₅₀ value of 5.8 microns.

實例3：Example 3:

將來自Evonik Degussa GmbH之磨料牙膏矽石9如實例2中以根據本發明之製程在來自Netzsch-Condux之CGS 50型流化床對向噴研磨機中研磨一次。另一選擇地，將9在來自Alpine之UPZ 160機械打擊式研磨機中研磨。具有約600公斤平均產出量，機械打擊式研磨機產製約6.5公克磨料，對應於增加11 ppm之鐵雜質。在根據本發明研磨之例子中，鐵雜質的增加少於1 ppm。Abrasive toothpaste vermiculite from Evonik Degussa GmbH 9 was milled once in Example 2 in a CGS 50 fluidized bed opposed jet mill from Netzsch-Condux in accordance with the process of the present invention. Another option, 9 Grinding in a UPZ 160 mechanical striking mill from Alpine. With an average output of approximately 600 kg, the mechanical impact mill produces 6.5 grams of abrasive, corresponding to an increase of 11 ppm of iron impurities. In the example of grinding according to the present invention, the increase in iron impurities is less than 1 ppm.

1．．．噴射研磨機1. . . Jet mill

2．．．圓筒狀容箱2. . . Cylindrical container

3．．．研磨室3. . . Grinding room

4．．．待研磨材料之進料4. . . Feed of material to be ground

5．．．研磨噴射入口5. . . Grinding jet inlet

6．．．產物出口6. . . Product export

7．．．空氣分級器7. . . Air classifier

8．．．分級輪8. . . Grading wheel

9．．．入口孔或入口噴嘴9. . . Inlet or inlet nozzle

10．．．研磨噴射流10. . . Grinding jet

11．．．加熱源11. . . Heating source

12．．．加熱源12. . . Heating source

13．．．饋入管13. . . Feed tube

14．．．溫度隔絕套14. . . Temperature isolation sleeve

15．．．入口15. . . Entrance

16．．．出口16. . . Export

17．．．研磨室中心17. . . Grinding chamber center

18．．．儲槽或產生裝置，優先選擇為鼓風機18. . . Storage tank or generating device, preferred as blower

19．．．引導裝置19. . . Guiding device

20．．．出口通孔20. . . Outlet through hole

21．．．分級器容箱twenty one. . . Grader container

22．．．容箱上部件twenty two. . . Container upper part

23．．．容箱下部件twenty three. . . Container lower part

24．．．周圍凸緣twenty four. . . Surrounding flange

25．．．周圍凸緣25. . . Surrounding flange

26．．．活節接頭26. . . Joint joint

27．．．箭號27. . . Arrow

28．．．分級室容箱28. . . Grading room container

28a．．．支撐臂28a. . . Support arm

29．．．排放錐體29. . . Emission cone

30．．．凸緣30. . . Flange

31．．．凸緣31. . . Flange

32．．．蓋板32. . . Cover

33．．．蓋板33. . . Cover

34．．．葉片34. . . blade

35．．．分級輪軸35. . . Grading wheel

35a．．．旋轉軸承35a. . . Rotary bearing

36．．．上機製板36. . . Upper mechanism board

37．．．下機製板37. . . Lower mechanism board

38．．．容箱末端部位38. . . End of the tank

39．．．產物進料通孔39. . . Product feed through hole

40．．．旋轉軸40. . . Rotary axis

41．．．出口室41. . . Exit room

42．．．上蓋板42. . . Upper cover

43．．．可拆卸蓋43. . . Detachable cover

44．．．支撐臂44. . . Support arm

45．．．圓錐形環狀容箱45. . . Conical ring box

46．．．進氣過濾器46. . . Intake filter

47．．．穿孔板47. . . Perforated plate

48．．．細料排放管48. . . Fine material discharge pipe

49．．．偏向錐體49. . . Biased cone

50．．．分級空氣入口螺旋50. . . Graded air inlet spiral

51．．．粗粒材料排放51. . . Coarse material discharge

52．．．凸緣52. . . Flange

53．．．凸緣53. . . Flange

54．．．分散區54. . . Dispersed area

55．．．在內緣及內襯上經機械加工(成斜面)之凸緣55. . . Machined (beveled) flange on the inner edge and inner lining

56．．．可交換之保護管56. . . Exchangeable protection tube

57．．．可交換之保護管57. . . Exchangeable protection tube

58．．．細料出口58. . . Fine material export

59．．．葉片環59. . . Blade ring

本發明僅以參考圖式之示例性具體例為基準的實例方式更詳細解釋於下，其中The present invention is explained in more detail below by way of example with reference to an exemplary embodiment of the drawings, wherein

圖1係以圖式顯示呈部分截面示意圖的噴射研磨機之示例性具體例。BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a view showing an exemplary embodiment of a jet mill in a partial sectional view.

圖2顯示呈垂直配置且呈示意之中心縱截面的噴射研磨機之空氣分級器的示例性具體例，分級輪指配用於分級空氣與固體粒子之混合物的出口管，及2 shows an exemplary embodiment of an air classifier of a jet mill in a vertical configuration and having a schematic central longitudinal section, the classifying wheel being assigned an outlet pipe for classifying a mixture of air and solid particles, and

圖3顯示以示意圖像且呈垂直截面的空氣分級器之分級輪。Figure 3 shows a grading wheel of an air classifier with a schematic image and a vertical cross section.

1．．．噴射研磨機1. . . Jet mill

2．．．圓筒狀容箱2. . . Cylindrical container

3．．．研磨室3. . . Grinding room

4．．．待研磨材料之進料4. . . Feed of material to be ground

5．．．研磨噴射入口5. . . Grinding jet inlet

6．．．產物出口6. . . Product export

7．．．空氣分級器7. . . Air classifier

8．．．分級輪8. . . Grading wheel

9．．．入口孔或入口噴嘴9. . . Inlet or inlet nozzle

10．．．研磨噴射流10. . . Grinding jet

11．．．加熱源11. . . Heating source

12．．．加熱源12. . . Heating source

13．．．饋入管13. . . Feed tube

14．．．溫度隔絕套14. . . Temperature isolation sleeve

15．．．入口15. . . Entrance

16．．．出口16. . . Export

17．．．研磨室中心17. . . Grinding chamber center

18．．．儲槽或產生裝置，優先選擇為鼓風機18. . . Storage tank or generating device, preferred as blower

18a．．．槽18a. . . groove

19．．．引導裝置19. . . Guiding device

40．．．旋轉軸40. . . Rotary axis

Claims (11)

一種產生材料細粒子之製程，其包括：將該材料饋至噴射研磨機之研磨室；使用旋轉式鼓風機或徑向式鼓風機產生研磨氣體介質，並將所產生的研磨氣體介質經由至少一個流體噴嘴導入該研磨室中；於該研磨室中使該材料與該研磨氣體介質碰撞，以得到含粗粒與細粒之研磨產物；將該研磨產物送至動態空氣分級器；於該動態空氣分級器中分離該粗粒與該細粒；自該動態空氣分級器中移出該細粒，並收集該細粒；以及將該粗粒送回該研磨室；其中，該研磨氣體介質具有≦4巴之壓力(絕對)及該研磨氣體介質具有低於100℃之溫度。 A process for producing fine particles of a material, comprising: feeding the material to a grinding chamber of a jet mill; generating a grinding gas medium using a rotary blower or a radial blower, and passing the generated abrasive gas medium through at least one fluid nozzle Introducing into the grinding chamber; colliding the material with the grinding gas medium in the grinding chamber to obtain a ground product containing coarse particles and fine particles; sending the ground product to a dynamic air classifier; and the dynamic air classifier Separating the coarse particles from the fine particles; removing the fine particles from the dynamic air classifier, and collecting the fine particles; and returning the coarse particles to the grinding chamber; wherein the grinding gas medium has a crucible of 4 bar The pressure (absolute) and the abrasive gas medium have a temperature below 100 °C. 根據申請專利範圍第1項之製程，其中該噴射研磨機為橢圓管研磨機或螺旋管噴射研磨機。 According to the process of claim 1, wherein the jet mill is an elliptical tube mill or a spiral tube jet mill. 根據申請專利範圍第1項之製程，其中該噴射研磨機為整合有動態空氣分級器之流化床對向噴射研磨機或密相床噴射研磨機。 According to the process of claim 1, wherein the jet mill is a fluidized bed opposed jet mill or a dense bed jet mill integrated with a dynamic air classifier. 根據申請專利範圍第3項之製程，其中該動態空氣分級器包括具有固定或隨半徑減少而增加之淨高的分級轉子或分級輪(8)，使得操作期間流經的分級轉子或分級輪(8)的表面積至少大致固定。 According to the process of claim 3, wherein the dynamic air classifier comprises a classifying rotor or classifying wheel (8) having a net height that is fixed or increased with decreasing radius, such that a graded rotor or a classifying wheel flows during operation ( 8) The surface area is at least substantially fixed. 根據申請專利範圍第3或4項之製程，其中該動態空氣分級器包括具有浸沒管(20)的分級轉子或分級輪(8)，該浸沒管係以分級轉子或分級輪(8)旋轉時隨著其一起旋轉的方式設計。 The process according to claim 3, wherein the dynamic air classifier comprises a classifying rotor or a classifying wheel (8) having a immersion tube (20), the immersion tube being rotated by a classifying rotor or a classifying wheel (8) Designed as it rotates together. 根據申請專利範圍第3或4項之製程，其中該細料通過動態空氣分級器的一細料出口室(41)，及該細料出口室具有在流動方向上變寬的橫截面。 According to the process of claim 3 or 4, wherein the fine material passes through a fine material outlet chamber (41) of the dynamic air classifier, and the fine material outlet chamber has a cross section which widens in the flow direction. 根據申請專利範圍第1至4項中任一項之製程，其中研磨氣體介質包括至少一種選自空氣、氬氣、氦氣、氮氣及其他惰性氣體之氣體。 The process of any one of claims 1 to 4 wherein the abrasive gas medium comprises at least one gas selected from the group consisting of air, argon, helium, nitrogen, and other inert gases. 根據申請專利範圍第1至4項中任一項之製程，另包括：在研磨期間加入塗料或摻雜劑；其中待研磨材料之粒子的至少部分表面被塗料或摻雜劑覆蓋。 The process according to any one of claims 1 to 4, further comprising: adding a coating or a dopant during the grinding; wherein at least part of the surface of the particles of the material to be ground is covered by the coating or the dopant. 根據申請專利範圍第1至4項中任一項之製程，其中該研磨氣體介質的溫度低於或等於95℃。 The process of any one of claims 1 to 4 wherein the temperature of the abrasive gas medium is less than or equal to 95 °C. 根據申請專利範圍第1至4項中任一項之製程，其中該研磨氣體介質的壓力低於3巴。 The process of any one of claims 1 to 4 wherein the pressure of the abrasive gas medium is less than 3 bar. 根據申請專利範圍第9項之製程，其係以研磨氣體介質壓力與溫度的以下組合操作：0.15至0.5巴及50至80℃。 According to the process of claim 9 of the patent application, it is operated in the following combination of the pressure of the grinding gas medium and the temperature: 0.15 to 0.5 bar and 50 to 80 °C.